CN105692601A - Method for preparing graphene blocks and graphene blocks prepared by same - Google Patents
Method for preparing graphene blocks and graphene blocks prepared by same Download PDFInfo
- Publication number
- CN105692601A CN105692601A CN201610054220.1A CN201610054220A CN105692601A CN 105692601 A CN105692601 A CN 105692601A CN 201610054220 A CN201610054220 A CN 201610054220A CN 105692601 A CN105692601 A CN 105692601A
- Authority
- CN
- China
- Prior art keywords
- graphene
- bulk
- preparation
- graphene oxide
- blocks
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Abstract
The invention provides a method for preparing graphene blocks. According to the method provided by the invention, a plurality of graphene oxide films are heated at high pressure under the action of a binding aid to form graphene blocks. According to the method for preparing the graphene blocks, graphene oxide is used as a raw material to prepare highly-oriented graphene heat-conduction blocks, and each of the highly-oriented graphene heat-conduction blocks can be made to be larger in size to reach a volume over 400*400*400mm, instead of highly-oriented pyrolytic graphite. The method provided by the invention is simple in process, short in preparation cycle, low in cost and more widely applied.
Description
Technical field
The present invention relates to field of electronic materials, the preparation method particularly relating to a kind of Graphene bulk and the product obtained。
Background technology
Highly oriented pyrolytic graphite, has highly oriented laminated structure, has the significantly high coefficient of heat conduction in x-y face, it is possible to as heat conduction functional material, play the effect of body surface equalizing temperature。But highly oriented pyrolytic graphite complicated process of preparation, expensive, its application is extremely restricted。
Accordingly, it is desirable to provide a kind of simpler easy preparation method, obtain the Graphene bulk of highly directional heat conduction。
Summary of the invention
The preparation method that the present invention proposes a kind of Graphene bulk, technique is simple, and the manufacturing cycle is short, is widely used。
The technical scheme is that and be achieved in that: the preparation method of a kind of Graphene bulk, by by several graphene oxide films under the effect of adhesive aid, form Graphene bulk through hyperbaric heating。
Further, described graphene oxide film adopts wet-layer preparation to obtain, and is namely prepared by steps such as dispersion, filtering coatings。
Further, described wet-layer preparation includes: be dispersed in diluent by graphene oxide, and wherein the mass content of graphene oxide is 0.5%-10%, forms graphene oxide slurry, described Graphene slurry is coated on base material, and be dried, obtain graphene oxide film, wherein, described base material can adopt PET, stainless steel band etc., because graphene oxide is a two-dimentional material, in dry run, graphene oxide can arrange along with the volatilization automatic orientation of solvent。
Further, graphene oxide film owing to obtaining in above-mentioned steps only has 20 ~ 200 μm, very thin, the bulk that thickness processed is very thick, need to stack much opening graphene oxide film, adding auxiliary agent in the middle of every layer of graphene oxide film, described adhesive aid includes one or more in organosilicon, titanium compound, aluminium compound etc.。
Further, autoclave process is under the protection of protective gas, and pressurize 50-100kg/cm2, heating, to 1300-2000 DEG C, is reduced, the functional group of surface of graphene oxide is removed completely, obtain Graphene bulk, and wherein, protective gas can adopt nitrogen。
Further, in order to improve heat conductivity further, after autoclave process, also include graphitization。
Further, described graphite turns to the Graphene bulk that obtains in graphitizing furnace, is warming up to 2800-3000 DEG C and carries out graphitization, and the Graphene bulk finally given has heat conductivity in x-y face and reaches 1500W/m K。
By the Graphene bulk that said method obtains。
The preparation method of the described Graphene bulk of the present invention, use graphene oxide is raw material, prepare high starch breeding alkene heat-conducting block, it is very big that size can be done, reaching the volume of more than 400*400*400mm, replace highly oriented pyrolytic graphite, the technique simple manufacturing cycle is short, low price, applies more extensive。
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, the accompanying drawing used required in embodiment or description of the prior art will be briefly described below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings。
Fig. 1 is the process flow diagram of the preparation method of a kind of Graphene bulk of the present invention。
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention, rather than whole embodiments。Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention。
Embodiment 1
Being dispersed in 99kg water by 1kg graphene oxide, preparation is the graphene oxide slurry of 1% solid content；Sieve de-bubbled, then use coating equipment coating 3mm by the above-mentioned slurry prepared, the dry graphene oxide film obtaining 30 μ m thick；At dry graphene oxide film two sides spraying polysiloxanes；Being then cut into the square of 150mm × 150mm, 1000 stack；Then using hot pressing furnace pressurized, heated to reduce, pressurize 50kg/cm2, is heated to 1500 DEG C；Bulk obtained above is re-used graphitizing furnace, is heated to 2900 DEG C, carry out graphitization；Finally giving the high starch breeding alkene heat-conducting block of 150mm × 150mm × 6mm, density is 2.2g/cm3, and heat conductivity reaches 1500W/m K。
Embodiment 2
Being dispersed in the NMP of 97kg by 3kg graphene oxide, preparation is the graphene oxide slurry of 3% solid content；Sieve de-bubbled, then use coating equipment coating 3mm by the above-mentioned slurry prepared, the dry graphene oxide film obtaining 100 μ m thick；At dry graphene oxide film two sides spraying TiO2；Being then cut into the square of 150mm × 150mm, 1000 stack；Then using hot pressing furnace pressurized, heated to reduce, pressurize 100kg/cm2, is heated to 1700 DEG C；Bulk obtained above is re-used graphitizing furnace, is heated to 3000 DEG C, carry out graphitization；Finally giving the high starch breeding alkene heat-conducting block of 150mm × 150mm × 18mm, density is 2.2g/cm3, and heat conductivity reaches 1500W/m K。
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention。
Claims (8)
1. the preparation method of a Graphene bulk, it is characterised in that: by by several graphene oxide films under the effect of adhesive aid, through hyperbaric heating formed Graphene bulk。
2. the preparation method of Graphene bulk as described in the appended claim 1, it is characterised in that: described graphene oxide film adopts wet-layer preparation to obtain。
3. the preparation method of Graphene bulk as stated in claim 2, it is characterized in that: described wet-layer preparation includes: graphene oxide is dispersed in diluent, wherein the mass content of graphene oxide is 0.5%-10%, form graphene oxide slurry, described Graphene slurry is coated on base material, and be dried, obtain graphene oxide film。
4. the preparation method of Graphene bulk as described in the appended claim 1, it is characterised in that: described adhesive aid includes one or more in organosilicon, titanium compound, aluminium compound。
5. the preparation method of Graphene bulk as described in the appended claim 1, it is characterised in that: autoclave process is under the protection of protective gas, and pressurize 50-100kg/cm2, the functional group of surface of graphene oxide, to 1300-2000 DEG C, is removed, obtains Graphene bulk by heating completely。
6. the preparation method of Graphene bulk as claimed in claim 5, it is characterised in that: after autoclave process, also include graphitization。
7. the preparation method of Graphene bulk as recited in claim 6, it is characterised in that: described graphite turns to the Graphene bulk that obtains in graphitizing furnace, is warming up to 2800-3000 DEG C and carries out graphitization。
8. the Graphene bulk prepared by either method in claim 1-7。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610054220.1A CN105692601B (en) | 2016-01-27 | 2016-01-27 | A kind of preparation method of graphene bulk and obtained graphene bulk |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610054220.1A CN105692601B (en) | 2016-01-27 | 2016-01-27 | A kind of preparation method of graphene bulk and obtained graphene bulk |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105692601A true CN105692601A (en) | 2016-06-22 |
| CN105692601B CN105692601B (en) | 2018-07-10 |
Family
ID=56228539
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610054220.1A Active CN105692601B (en) | 2016-01-27 | 2016-01-27 | A kind of preparation method of graphene bulk and obtained graphene bulk |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105692601B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107585763A (en) * | 2017-10-23 | 2018-01-16 | 南京旭羽睿材料科技有限公司 | A kind of graphene particles and preparation method thereof |
| CN108819400A (en) * | 2018-06-26 | 2018-11-16 | 青岛科技大学 | A method of anisotropic thermal block materials are prepared using Gibbs free energy induction |
| WO2018219008A1 (en) * | 2017-05-27 | 2018-12-06 | 杭州高烯科技有限公司 | Method for preparing composites on basis of graphene bonding |
| CN109694055A (en) * | 2018-12-28 | 2019-04-30 | 常州富烯科技股份有限公司 | High-density graphite alkene foam film and preparation method thereof |
| CN110077048A (en) * | 2019-05-16 | 2019-08-02 | 重庆云天化瀚恩新材料开发有限公司 | A kind of graphene heat-conducting piece and preparation method thereof |
| CN110511029A (en) * | 2019-09-10 | 2019-11-29 | 北京中石伟业科技无锡有限公司 | A kind of method that binder free graphene oxide prepares high orientation graphite block body |
| CN112723345A (en) * | 2021-03-26 | 2021-04-30 | 云南云天墨睿科技有限公司 | Composite graphene slurry with self-assembly property and preparation method thereof |
| CN112794716A (en) * | 2020-12-31 | 2021-05-14 | 云南云天墨睿科技有限公司 | Graphene membrane material with specified thickness and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449423A (en) * | 2013-08-27 | 2013-12-18 | 常州第六元素材料科技股份有限公司 | Graphene heat conducting membrane and preparation method thereof |
| CN103770433A (en) * | 2012-10-18 | 2014-05-07 | 绿晶能源股份有限公司 | Artificial graphite heat radiation substrate and making method thereof |
| CN104609405A (en) * | 2015-01-09 | 2015-05-13 | 上海大学 | Preparation method of vertically arrayed graphene thin films |
-
2016
- 2016-01-27 CN CN201610054220.1A patent/CN105692601B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103770433A (en) * | 2012-10-18 | 2014-05-07 | 绿晶能源股份有限公司 | Artificial graphite heat radiation substrate and making method thereof |
| CN103449423A (en) * | 2013-08-27 | 2013-12-18 | 常州第六元素材料科技股份有限公司 | Graphene heat conducting membrane and preparation method thereof |
| CN104609405A (en) * | 2015-01-09 | 2015-05-13 | 上海大学 | Preparation method of vertically arrayed graphene thin films |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018219008A1 (en) * | 2017-05-27 | 2018-12-06 | 杭州高烯科技有限公司 | Method for preparing composites on basis of graphene bonding |
| CN107585763A (en) * | 2017-10-23 | 2018-01-16 | 南京旭羽睿材料科技有限公司 | A kind of graphene particles and preparation method thereof |
| CN107585763B (en) * | 2017-10-23 | 2018-10-19 | 南京旭羽睿材料科技有限公司 | A kind of graphene particles and preparation method thereof |
| CN108819400A (en) * | 2018-06-26 | 2018-11-16 | 青岛科技大学 | A method of anisotropic thermal block materials are prepared using Gibbs free energy induction |
| CN109694055A (en) * | 2018-12-28 | 2019-04-30 | 常州富烯科技股份有限公司 | High-density graphite alkene foam film and preparation method thereof |
| CN109694055B (en) * | 2018-12-28 | 2021-12-03 | 常州富烯科技股份有限公司 | High-density graphene foam film and preparation method thereof |
| CN110077048A (en) * | 2019-05-16 | 2019-08-02 | 重庆云天化瀚恩新材料开发有限公司 | A kind of graphene heat-conducting piece and preparation method thereof |
| CN110511029A (en) * | 2019-09-10 | 2019-11-29 | 北京中石伟业科技无锡有限公司 | A kind of method that binder free graphene oxide prepares high orientation graphite block body |
| CN112794716A (en) * | 2020-12-31 | 2021-05-14 | 云南云天墨睿科技有限公司 | Graphene membrane material with specified thickness and preparation method thereof |
| CN112723345A (en) * | 2021-03-26 | 2021-04-30 | 云南云天墨睿科技有限公司 | Composite graphene slurry with self-assembly property and preparation method thereof |
| CN112723345B (en) * | 2021-03-26 | 2023-09-29 | 云南云天墨睿科技有限公司 | Composite graphene slurry with self-assembly property and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105692601B (en) | 2018-07-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105692601A (en) | Method for preparing graphene blocks and graphene blocks prepared by same | |
| CN104553102B (en) | Superhigh temperature gradient heat-barrier material and preparation method thereof | |
| CN109354823B (en) | Preparation method of heat-insulation ceramizable phenolic resin-based gradient composite material | |
| CN107973290A (en) | Elastic graphite alkene Heat Conduction Material and preparation method thereof | |
| CN104876616B (en) | A kind of high temperature resistant absorbing material and preparation method thereof | |
| CN109517520A (en) | A kind of aeroge coating, airsetting gel coating and the method by aeroge coating preparation airsetting gel coating | |
| CN109971020B (en) | Functional nano cellulose-boron nitride composite film and preparation method thereof | |
| CN103058712A (en) | C/SiC composite coating applied to surface of low-density carbon/carbon composite material and preparation process thereof | |
| CN102515850A (en) | Carbon/carbon composite material ultrahigh temperature oxidation resistant coating and preparation method thereof | |
| US8916239B2 (en) | Flexible graphite sheet and method for fabricating the same and composite structure for the same | |
| CN107032796A (en) | Self-healing SiC/ZrSi2‑MoSi2Coating material and preparation method | |
| CN102584240A (en) | Sintering method of ZrB2-SiC superhigh temperature ceramics | |
| CN106555093A (en) | A kind of CNT strengthens aluminum silicon carbide composite material and preparation method thereof | |
| CN109824382A (en) | A kind of heat management SiC/ graphite film laminar composite and preparation method thereof | |
| CN107129298B (en) | graphene/ZrO2Method for preparing ceramic composite material | |
| CN103232257A (en) | Fast connection method of carbon/carbon composite material | |
| Kong et al. | Effects of plasma treatment on properties of carbon fiber and its reinforced resin composites | |
| JP2020521712A (en) | High thermal conductivity polyimide-based composite carbon film and method for producing the same | |
| CN114394586A (en) | Method for preparing graphene temperature-uniforming plate through vacuum thermal sintering | |
| CN106675360B (en) | Antistatic polyether ketone ketone powdery paints and preparation method thereof | |
| CN106631080B (en) | A kind of preparation method of Si-O-C ceramics flexible base board | |
| CN106752804B (en) | High temperature resistant, antistatic polyether ketone ketone powdery paints and preparation method thereof | |
| CN106588121B (en) | A kind of preparation method of SiC nanowire and SiC-MoSi2-CrSi2 coating symbiosis length | |
| CN106179923B (en) | The preparation method of graphene metallic composite | |
| CN109437942A (en) | A kind of light pyrolysis adaptively ties up the efficient heat insulation material of shape |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |